CN104925867A - Nano cesium tungstate powder and preparing method and application of nano cesium tungstate powder - Google Patents
Nano cesium tungstate powder and preparing method and application of nano cesium tungstate powder Download PDFInfo
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Abstract
The invention discloses nano cesium tungstate powder and a preparing method and application of the nano cesium tungstate powder. According to the method, the nano cesium tungstate powder is prepared through the ultrasonic chemical method, and the obtained nano cesium tungstate powder is small in particle size, evenly dispersed, small in aggregation and high in purity. In addition, the synthesis technique is simple and efficient, raw materials can be obtained easily, reproducibility is high, and industrialization is facilitated. Furthermore, the nano cesium tungstate powder obtained through the method is suitable for heat insulation and heat preservation of buildings and automotive glass, the heat insulation effect is good while high visible light transmittance can be guaranteed, and the nano cesium tungstate powder has good cost advantages and broad development prospects.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly relate to a kind of nanometer wolframic acid caesium powder and preparation method thereof and application.
Background technology
Wolframic acid caesium (Cs
2wO
4) be the novel material be just found in recent years, the famous paint company such as some Japan, Germany, U.S. all greatly develops the transparent heat insulating dope of wolframic acid caesium at present.Nanometer wolframic acid caesium powder is a kind of inorganic nanometer powder near infrared to optimal absorption ability, it not only has extremely strong absorption characteristic near infrared region (wavelength is 800 ~ 1100nm), have stronger through characteristic visible region (wavelength is 380 ~ 780nm) simultaneously, and UV light region (wavelength is 200 ~ 380nm), also there is stronger shielding character.Because nanometer wolframic acid caesium powder has outstanding near infrared absorption, visible transmission feature, so, the conglomerate field such as automobile adhesive film, sunshading and heat-insulating, pattern plastic warmhouse booth heat insulation at building glass has broad application prospects.
But the current domestic research prepared about nanometer wolframic acid caesium powder is less, wherein mainly contains the preparation methods such as solid phase method, liquid-phase coprecipitation, microemulsion method, hydrothermal method.But there is many deficiencies such as cost is higher, production efficiency is low in manufacture process in above-mentioned preparation method, but also it is large to there is product grain, lack of homogeneity, is difficult to the requirement reaching transmitance more than 70%, the problems such as Film Haze is greater than 3%, and coating quality is poor, dispersion efficiency is low.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of nanometer wolframic acid caesium powder and preparation method thereof and application, be intended to solve the problem that product dispersiveness is poor, thermal insulation is poor and visible light transmissivity is low prepared by existing preparation method.
Technical scheme of the present invention is as follows:
A kind of nanometer wolframic acid caesium raw powder's production technology, wherein, comprises step:
A, according to n (Cs)/n (W)=0.33:1, tungsten salt and cesium salt to be dissolved in citric acid solution and alcoholic solvent, after stirring, to react 2 ~ 3 hours under 180-200 DEG C of condition, obtain tungsten, caesium mixed solution;
B, in tungsten, caesium mixed solution, add appropriate urea, regulate pH value to 3 ~ 5 of reaction solution, be stirred to urea and dissolve completely;
C, the mixed solution argon gas after dissolving completely in step B to be washed, and carry out chemical reaction 2 ~ 6h through Ultrasonic Radiation under 70 ~ 90 DEG C and argon shield, obtain gelatinous precipitate;
D, gelatinous precipitate carried out ageing 4 ~ 24h, carries out afterwards filtering, wash, wash after carry out drying, finally calcine, obtain nanometer wolframic acid caesium powder.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described steps A, described tungsten salt is the one in sodium wolframate, ammonium tungstate, ammonium paratungstate, ammonium metawolframate; Described cesium salt is the one in cesium carbonate, cesium sulfate, cesium nitrate, cesium hydroxide.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described steps A, described alcoholic solvent is the one in methyl alcohol, ethanol, n-propyl alcohol, Virahol.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described step B, wolframic acid caesium molecular formula is Cs
2wO
4, the consumption of described urea is n(urea) and=n (Cs
1+)+6n (W
6+).
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described step C, the Ultrasonic Radiation frequency that described Ultrasonic Radiation adopts is 20.81kHz, 24.45kHz, 30.10kHz or 40.34kHz.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described step D, the detailed process of described filtration, washing is: adopt decompress filter, use distilled water wash gelatinous precipitate twice simultaneously, again with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally with dehydrated alcohol or deionized water wash twice.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described step D, the mode of described drying is forced air drying, vacuum-drying, lyophilize or microwave drying.
Described nanometer wolframic acid caesium raw powder's production technology, wherein, in described step D, the temperature of described calcining is 600 ~ 700 DEG C, and the time of calcining is 3 ~ 5h.
A kind of nanometer wolframic acid caesium powder, wherein, described nanometer wolframic acid caesium powder adopts as above arbitrary described nanometer wolframic acid caesium raw powder's production technology to be prepared from.
An application for nanometer wolframic acid caesium powder, wherein, is used for building the heat-insulation and heat-preservation with vehicle glass by nanometer wolframic acid caesium powder described above.
Beneficial effect: the present invention adopts such scheme, the nanometer wolframic acid caesium diameter of particle obtained is little, be uniformly dispersed, reunite less, purity is high.And synthesis technique of the present invention is simple, efficient, raw material is easy to get, favorable reproducibility, is conducive to industrialization.
Accompanying drawing explanation
Fig. 1 is the schema of a kind of nanometer wolframic acid of the present invention caesium raw powder's production technology preferred embodiment.
Fig. 2 is the X-ray diffraction spectrogram of embodiment 1 nanometer wolframic acid caesium powder.
Fig. 3 is the transmission electron microscope spectrogram of embodiment 1 nanometer wolframic acid caesium powder.
Fig. 4 is the size distribution test pattern of embodiment 1 nanometer wolframic acid caesium powder.
Embodiment
The invention provides a kind of nanometer wolframic acid caesium powder and preparation method thereof and application, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, Fig. 1 is the schema of a kind of nanometer wolframic acid of the present invention caesium raw powder's production technology preferred embodiment, and as shown in the figure, it comprises step:
S100, according to n (Cs)/n (W)=0.33:1, tungsten salt and cesium salt to be dissolved in citric acid solution and alcoholic solvent, after stirring, to react 2 ~ 3 hours under 180-200 DEG C of condition, obtain tungsten, caesium mixed solution;
S200, in tungsten, caesium mixed solution, add appropriate urea, regulate pH value to 3 ~ 5 of reaction solution, be stirred to urea and dissolve completely;
S300, the mixed solution argon gas after dissolving completely in step S200 to be washed, and carry out chemical reaction 2 ~ 6h through Ultrasonic Radiation under 70 ~ 90 DEG C and argon shield, obtain gelatinous precipitate;
S400, gelatinous precipitate carried out ageing 4 ~ 24h, carries out afterwards filtering, wash, wash after carry out drying, finally calcine, obtain nanometer wolframic acid caesium powder.
The present invention adopts sonochemistry legal system for nanometer wolframic acid caesium powder, compared with preparing nanometer wolframic acid caesium powder with preparation methods such as existing solid phase method, liquid-phase coprecipitation, microemulsion method, hydrothermal methods, the particle diameter of nanometer powder that preparation method of the present invention prepares is little, be uniformly dispersed, reunite less, purity is high; And preparation method of the present invention is simple, efficient, favorable reproducibility, is conducive to industrialization.
Preferably, in described step S100, the collocation method of described citric acid solution is: be added in appropriate deionized water by appropriate citric acid.The concentration of described citric acid solution is 1-5mol/L.
Preferably, in described step S100, described tungsten salt is the one in sodium wolframate, ammonium tungstate, ammonium paratungstate, ammonium metawolframate; Described cesium salt is the one in cesium carbonate, cesium sulfate, cesium nitrate, cesium hydroxide; Described alcoholic solvent is the one in methyl alcohol, ethanol, n-propyl alcohol, Virahol.More preferably, described tungsten salt is sodium wolframate; Described cesium salt is cesium carbonate; Alcoholic solvent is methyl alcohol.With described sodium wolframate and cesium carbonate for raw material, methyl alcohol is solvent, reacts 2 ~ 3 hours, can obtain uniform tungsten, caesium mixed solution under the effect of citric acid reductive agent at 180-200 DEG C.And cheaper starting materials of the present invention, gentleness are easy to operate, effectively can reduce production cost, be applicable to large-scale industrial production.
Preferably, in described step S200, wolframic acid caesium molecular formula is Cs
2wO
4, the consumption of described urea is n(urea) and=n (Cs
1+)+6n (W
6+); In described step S200, can improve the agglomeration traits of the nano-powder of formation by controlling reaction pH, reaction system terminal pH value is 3 ~ 5, and temperature of reaction is 50 ~ 80 DEG C.
In described step S300, after the mixed solution after dissolving completely is stirred, with argon gas washing 10 ~ 30min, and carry out chemical reaction 2 ~ 6h through Ultrasonic Radiation under 70 ~ 90 DEG C and argon shield, obtain gelatinous precipitate in step S200.The present invention adopts hyperacoustic method to react, and is beneficial to formation good dispersity, few target product of reuniting.
Preferably, in described step S300, the Ultrasonic Radiation frequency that described Ultrasonic Radiation adopts is 20.81kHz, 24.45kHz, 30.10kHz or 40.34kHz.Ultrasonic wave of the present invention has the function of frequency-adjustable, when frequency is bigger than normal, the dispersion of the mixed solution of reaction evenly, reunite less.Preferably, described Ultrasonic Radiation frequency is 30.10kHz, to guarantee the dispersion effect of mixed solution further.
Preferably, in described step S400, the detailed process of described filtration, washing is: adopt decompress filter, use distilled water wash gelatinous precipitate twice simultaneously, again with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally with dehydrated alcohol or deionized water wash twice.
Preferably, in described step S400, the mode of described drying can be forced air drying, vacuum-drying, lyophilize or microwave drying etc.More preferably, the mode of described drying is vacuum-drying.
Preferably, in described step S400, the temperature of described calcining is 600 ~ 700 DEG C, and the time of calcining is 3 ~ 5h.More preferably, the temperature of described calcining is 650 DEG C, and the time of calcining is 4h.
Based on aforesaid method, the present invention also provides a kind of nanometer wolframic acid caesium powder, and described nanometer wolframic acid caesium powder adopts as above arbitrary described nanometer wolframic acid caesium raw powder's production technology to be prepared from.The present invention adopts sonochemistry method, makes the wolframic acid caesium nano-powder prepared have decentralized good, reproducible excellent properties; And preparation technology's equipment of the present invention is simple, cheaper starting materials is easy to get, and therefore has vast potential for future development.
Based on aforesaid method, the present invention also provides a kind of application of nanometer wolframic acid caesium powder, and nanometer wolframic acid caesium powder described above is used for building the heat-insulation and heat-preservation with vehicle glass.Nanometer wolframic acid caesium powder of the present invention is applicable to the heat-insulation and heat-preservation of building and vehicle glass, and can while guarantee has higher visible light transmissivity, and good heat-insulation effect, also has better cost advantage.
With specific embodiment, the present invention is elaborated below:
Embodiment 1
1), get sodium wolframate and 0.977 cesium carbonate of 1.47g, add citric acid solution and methanol reagent that concentration is 3mol/L, stir, react 3 hours under 200 DEG C of conditions, obtain tungsten, caesium mixed solution;
2), by tungsten, caesium mixed solution add the urea of 1.98g, regulate the pH value to 4 of reaction solution, be stirred to urea and dissolve completely, form clear solution;
3), stir above-mentioned solution wash 10min with argon gas after evenly, then under 70 DEG C and argon shield, insert ultrasonic wave inserting tube, be the Ultrasonic Radiation 4h of 20.81kHz by frequency, obtain gelatinous precipitate;
4), by gelatinous precipitate through ageing 5h, after filtration under diminished pressure, and with distilled water wash twice, then with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally use absolute ethanol washing twice; By gained presoma grind into powder after dry a few hours at 80 DEG C, powder is placed in retort furnace, and in 600 DEG C of insulation 3h, furnace cooling, can obtain target product nanometer wolframic acid caesium powder.
Target product nanometer wolframic acid caesium powder is characterized.Wherein, Fig. 2 is the X-ray diffraction spectrogram (XRD) of nanometer wolframic acid caesium powder; Fig. 3 is the transmission electron microscope spectrogram (TEM) of nanometer wolframic acid caesium powder; Fig. 4 is the size distribution test pattern of nanometer wolframic acid caesium powder.Interpretation of result finds: the nanometer wolframic acid caesium powder purity that the present invention obtains is high, be uniformly dispersed, reunite less, particle diameter is little.
Embodiment 2:
1), get the sodium wolframate of 1.18g and the cesium sulfate of 0.65g, add citric acid solution and ethanol reagent that concentration is 5mol/L, stir, react 2 hours under 180 DEG C of conditions, obtain tungsten, caesium mixed solution;
2), in tungsten, caesium mixed solution, add the urea of 1.56g, regulate the pH value to 3 of reaction solution, be stirred to urea and dissolve completely, form clear solution;
3), stir above-mentioned dissolution homogeneity after wash 10min with argon gas, then under 70 DEG C and argon shield, insert ultrasonic wave inserting tube, be the Ultrasonic Radiation 2h of 24.45kHz by frequency, obtain gelatinous precipitate;
4), by gelatinous precipitate through ageing 4h, after filtration under diminished pressure, and with distilled water wash twice, then with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally use absolute ethanol washing twice; By gained presoma grind into powder after dry a few hours at 80 DEG C, powder is placed in retort furnace, and in 700 DEG C of insulation 5h, furnace cooling, can obtain target product nanometer wolframic acid caesium powder.
XRD, TEM and the size distribution test pattern of the target product nanometer wolframic acid caesium powder of the present embodiment do not illustrate one by one at this.Find by analysis, the nanometer wolframic acid caesium powder that the present invention obtains have equally purity high, be uniformly dispersed, reunite less, advantage that particle diameter is little.
Embodiment 3:
1), get the ammonium paratungstate of 1.76g and the cesium nitrate of 1.30g, add citric acid solution and n-propyl alcohol reagent that concentration is 1mol/L, stir, react 2.5 hours under 190 DEG C of conditions, obtain tungsten, caesium mixed solution;
2), in tungsten, caesium mixed solution, add the urea of 2.4g, regulate the pH value to 5 of reaction solution, be stirred to urea and dissolve completely, form clear solution;
3), stir above-mentioned dissolution homogeneity after wash 30min with argon gas, then under 90 DEG C and argon shield, insert ultrasonic wave inserting tube, be the Ultrasonic Radiation 6h of 30.10kHz by frequency, obtain gelatinous precipitate;
4), by gelatinous precipitate through ageing 24h, after filtration under diminished pressure, and with distilled water wash twice, then with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally use absolute ethanol washing twice; By gained presoma grind into powder after dry a few hours at 80 DEG C, powder is placed in retort furnace, and in 650 DEG C of insulation 3h, furnace cooling, can obtain target product nanometer wolframic acid caesium powder.
XRD, TEM and the size distribution test pattern of the target product nanometer wolframic acid caesium powder of the present embodiment do not illustrate one by one at this.Find by analysis, the nanometer wolframic acid caesium powder that the present embodiment obtains still have purity high, be uniformly dispersed, reunite less, advantage that particle diameter is little.
In sum, a kind of nanometer wolframic acid caesium powder provided by the invention and preparation method thereof and application, the present invention adopts sonochemistry legal system for nanometer wolframic acid caesium powder, and the nanometer wolframic acid caesium diameter of particle obtained is little, be uniformly dispersed, reunite less, purity is high.And synthesis technique of the present invention is simple, efficient, raw material is easy to get, favorable reproducibility, is conducive to industrialization.In addition, nanometer wolframic acid caesium powder of the present invention is applicable to the heat-insulation and heat-preservation of building and vehicle glass, and can while guarantee has higher visible light transmissivity, and good heat-insulation effect, has better cost advantage, have vast potential for future development.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (10)
1. a nanometer wolframic acid caesium raw powder's production technology, is characterized in that, comprise step:
A, according to n (Cs)/n (W)=0.33:1, cesium salt and tungsten salt are dissolved in citric acid solution and alcoholic solvent, after stirring, react 2 ~ 3 hours under 180-200 DEG C of condition, obtain tungsten, caesium mixed solution;
B, in tungsten, caesium mixed solution, add appropriate urea, regulate pH value to 3 ~ 5 of reaction solution, be stirred to urea and dissolve completely;
C, the mixed solution argon gas after dissolving completely in step B to be washed, and carry out chemical reaction 2 ~ 6h through Ultrasonic Radiation under 70 ~ 90 DEG C and argon shield, obtain gelatinous precipitate;
D, gelatinous precipitate carried out ageing 4 ~ 24h, carries out afterwards filtering, wash, wash after carry out drying, finally calcine, obtain nanometer wolframic acid caesium powder.
2. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described steps A, described tungsten salt is the one in sodium wolframate, ammonium tungstate, ammonium paratungstate, ammonium metawolframate; Described cesium salt is the one in cesium carbonate, cesium sulfate, cesium nitrate, cesium hydroxide.
3. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described steps A, described alcoholic solvent is the one in methyl alcohol, ethanol, n-propyl alcohol, Virahol.
4. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described step B, wolframic acid caesium molecular formula is Cs
2wO
4, the consumption of described urea is n(urea) and=n (Cs
1+)+6n (W
6+).
5. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described step C, the Ultrasonic Radiation frequency that described Ultrasonic Radiation adopts is 20.81kHz, 24.45kHz, 30.10kHz or 40.34kHz.
6. nanometer wolframic acid caesium raw powder's production technology according to claim 1, it is characterized in that, in described step D, the detailed process of described filtration, washing is: adopt decompress filter, use distilled water wash gelatinous precipitate twice simultaneously, again with volume fraction be 10% ethanolic soln washing to filtrate in neutral, finally with dehydrated alcohol or deionized water wash twice.
7. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described step D, the mode of described drying is forced air drying, vacuum-drying, lyophilize or microwave drying.
8. nanometer wolframic acid caesium raw powder's production technology according to claim 1, is characterized in that, in described step D, the temperature of described calcining is 600 ~ 700 DEG C, and the time of calcining is 3 ~ 5h.
9. a nanometer wolframic acid caesium powder, is characterized in that, the nanometer wolframic acid caesium raw powder's production technology as described in described nanometer wolframic acid caesium powder employing is as arbitrary in claim 1-8 is prepared from.
10. an application for nanometer wolframic acid caesium powder, is characterized in that, nanometer wolframic acid caesium powder is as claimed in claim 9 used for building the heat-insulation and heat-preservation with vehicle glass.
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| CN106587157A (en) * | 2015-10-14 | 2017-04-26 | 易绍文 | Method for producing nano cesium tungstate powder |
| CN106587157B (en) * | 2015-10-14 | 2018-04-24 | 易绍文 | A kind of production method of nanometer of wolframic acid caesium powder |
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| CN107032403A (en) * | 2016-08-16 | 2017-08-11 | 海宁永欣科技咨询有限公司 | The processing technology of improved nanometer wolframic acid caesium powder |
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| CN106978005A (en) * | 2017-03-03 | 2017-07-25 | 厦门纳诺泰克科技有限公司 | A kind of tungstenic metal oxide nanoparticles and preparation method thereof |
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| CN108435195A (en) * | 2018-04-25 | 2018-08-24 | 辽宁科技学院 | A kind of preparation method and application of nanometer cobalt wolframic acid cesium salt |
| CN108435195B (en) * | 2018-04-25 | 2020-08-07 | 辽宁科技学院 | Preparation method and application of nano cobalt cesium tungstate |
| WO2021209289A1 (en) | 2020-04-15 | 2021-10-21 | Saint-Gobain Glass France | Vehicle glazing having a sun shade coating |
| CN115071026A (en) * | 2022-04-27 | 2022-09-20 | 嘉兴高正新材料科技股份有限公司 | Infrared high-barrier film and preparation method thereof |
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